US2956042A - Film forming compositions of polyethylene and polypropylene, film thereof, and method of making same - Google Patents

Film forming compositions of polyethylene and polypropylene, film thereof, and method of making same Download PDF

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US2956042A
US2956042A US702234A US70223457A US2956042A US 2956042 A US2956042 A US 2956042A US 702234 A US702234 A US 702234A US 70223457 A US70223457 A US 70223457A US 2956042 A US2956042 A US 2956042A
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film
polyethylene
polypropylene
weight
parts
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William F Underwood
Edward D Fuller
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Union Carbide Corp
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Union Carbide Corp
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene

Definitions

  • This invention relates to polyethylene film compositions. And, more particularly it relates to polyethylene film compositions exhibiting improved clarity.
  • Polyethylene in the form of seamless tubing or sheeting has found extensive use as a packaging, wrapping and covering material. Because it is inert to most chemi cals, possesses great mechanical strength, resists moisture vapor penetration and allows the material it protects to be seen, polyethylene film is admirably suited for these applications.
  • the films currently available although termed clear are characterized by a cloudiness, milkiness or haze.
  • a substantially homogeneous mixture of the polypropylene and polyethylene be achieved.
  • Intimate incorporation and dispersion can be obtained by the use of a differential two-roll mill, a Banbury mixer or similar apparatus.
  • the polyethylene is introduced into the mill or mixer, the desired amount of polypropylene is added and the two are mechanically worked until a substantially homogeneous mixture is obtained. Best results are obtained by carrying out the incorporation and dispersion of the polypropylene and polyethylene at a temperature equal to or above the melting point of the polyethylene.
  • Film-forming as used herein denotes a property of polyethylene whereby it can be formed into a self-sustaining film or employed as a surface coating. Any polyethylene which possesses this film-forming property is suitable for use in the composition of our invention. For example, polyethylene with a melt index of 1.9, and a density of 0.918 has given satisfactory results.
  • Polypropylene, suitable for use in this invention is total polymer made by the process disclosed in Australian patent application No. 6365/55 to Phillips Petroleum Company.
  • the total polymer comprises a tacky portion consisting of low molecular weight polymer, having a weight averaged molecular weight of from 500 to 5000, boiling above 900 F. and soluble at room tem perature in n-pentane and methyl isobutyl ketone; a solid portion consisting of high molecular weight polymer which also boils above 900 F. but which is insoluble in both n-pentane and methyl isobutyl ketone; and 10 to 20% of liquid polymeric material boiling at approximately 400 to 900 F.
  • the weight averaged molecular weight of the solid polymers ranges from between about 5000 and 20,000. These values were calculated according to the equation wherein M is the weight average molecular weight and N, is the intrinsic viscosity as determined for a solution of 0.2 gram of the polymer in 50 cc. of tetralin at 130 C. This type of molecular weight determination is de-' scribed by Dienis and Klemm, J. Applied Phys, 17, 458 (June 1946).
  • the proportion of polypropylene in polyethylene is critical. Improved clarity in a film can be obtained without substantially changing other physical characteristics by intimately incorporating and dispersing between 0.1 to 2.0 parts by weight of polypropylene in parts by weight of polyethylene. Amounts of polypropylene added in excess of 2.0 parts, although it improves the clarity of the film has the undesirable effect of imparting to the film a tacky and greasy feel. If an amount of polypropylene less than 0.1 part by weight of polypropylene in 100 parts by weight of polyethylene is used with the method of this invention there is no appreciable improve ment in clarity of the film produced therefrom.
  • the preferred limits of our invention are 0.5 to 1.5 parts by weight of polypropylene per 100 parts by weight of polyethylene.
  • any of the normally employed additives such as fillers, stabilizers, plasticizers, colorants and the like can be added to the composition of this invention provided they are not present in amounts which will offset the improvement in clarity rendered by the addition of the polypropylene.
  • the polyethylene-polypropylene mixture after removal from the mill or mixer can be melt extruded by any of the methods known to the art.
  • This invention is particularly suitable for the production of coatings or non-supported films of polyethylene with a thickness of between less than 0.0005 and about 0.005 in. and is especially useful for production of films for packaging applications where the advantage of transparency is desired in addition to the characteristic properties of polyethylene film such as in food wrapping, sales packages and see-through containers.
  • polyethyl ene with a molecular weight above 18,000 is placed on a differential two-roll mill and heated while it is being worked at a temperature equal to or greater than the melting point of the polyethylene i.e., about C.
  • the gradual addition of .5 to 1.5 parts by weight of polypropylene per 100 parts by weight of polyethylene is be gun.
  • the operation of the heated mill is not interrupted during the addition and is continued after the addition is completed and a substantially homogeneous mixture is obtained. This mixture is then removed from the mill, cooled and cut into particles of appropriate size for extrusion.
  • the preferred method of extrusion is the blown tube method disclosed in US. Patent 2,461,975 to Fuller and 2,461,976 to Schenk.
  • This method comprises, in general, dry extruding molten thermoplastic material through an annular die, in the form of a seamless tubing, and as the tubing is being drawn from the die, it is inflated to the desired diameter by means of an air bubble contained therein and a cooling medium applied to the periphery of the tubing.
  • the tubing is drawn continuously from the die and cooled until set whereupon it is flattened and wound on reels.
  • Sheeting can be made from the tubing by cutting one or both of the longitudinal edges.
  • Film produced from a polyethylene-polypropylene composition prepared without intimate incorporation and dispersion as achieved by heating the polyethylene to at least its melting point, as hereinbefore described does not exhibit the uniformly improved clarity which is characteristic of the composition which has been so processed.
  • EXAMPLE I removed from the mill, cooled and cut intb particles of a size suitable for melt extrusion.
  • the film was formed by the blown tube method of extrusion set forth in US. P. 2,461,976 and the clarity determined by ASTM method D-l003-52. The results of the test are given in terms of total surface haze.
  • the film prepared from the composition containing 0.5 part by weight polypropylene per 100 parts by weight polyethylene had a haze value of 2.1 units.
  • Example II Example I was repeated except that 1.0 parts by weight of polypropylene added per 100 parts by weight of polyethylene. The total surface haze of the film produced from this composition was found to be 2.6 units. The control sample again had a haze value of 6.7 units.
  • a method for the production of polyethylene film which includes the steps of intimately incorporating and dispersing in parts by weight of a normally solid film-forming ethylene polymer 0.1 to 2.0 parts by weight of polypropylene, and thereafter melt extruding the composition.
  • a method for the production of polyethylene film which includes the steps of intimately incorporating and dispersing in 100 parts by weight of a normally solid film-forming ethylene polymer 0.5 to 1.5 parts by weight of polypropylene, and thereafter melt extruding the composition.
  • a film-forming composition comprising a homo: geneous mixture of 100 parts by weight of a normally solid film-forming ethylene polymer and 0.1 to 2.0 parts by weight of polypropylene.
  • a film-forming composition comprising a homogeneous mixture of 100 parts by weight of a normally solid ethylene polymer and 05m 1.5 parts by weight of polypropylene.
  • a film-forming composition comprising a homogeneous mixture of 100 parts by weight of a normally solid ethylene polymer having a molecular weight greater than 18,000 and 0.5 to 1.5 parts by weight of polypropylene.
  • a transparent film comprising essentially a homogeneous mixture of 100 parts by weight of a normally solid, film-forming ethylene polymer and 0.1 to 2.0 parts by weight of polypropylene.
  • a transparent film comprising essentially a homogeneous mixture of 100 parts by weight of a normally solid, film-forming ethylene polymer and 0.5 to 1.5 parts by weight of polypropylene.
  • a transparent film comprising essentially a homogeneous mixture of 100 parts by weight of a normally solid, film-forming ethylene polymer having a molecular weight greater than 18,000 and 0.5 to 1.5 parts by weight of polypropylene.

Description

trite -.tes Pate Fatented Oct. 11,1960
William F. Underwood, Oak Park, and Edward D. Fuller, Chicago, Ill., assignor to Union Carbide Cor-' poration, a corporation of New York No Drawing. Filed Dec. 12, 1957, Ser. No. 702,234
Claims. (Cl. 260-455) This invention relates to polyethylene film compositions. And, more particularly it relates to polyethylene film compositions exhibiting improved clarity.
Polyethylene in the form of seamless tubing or sheeting has found extensive use as a packaging, wrapping and covering material. Because it is inert to most chemi cals, possesses great mechanical strength, resists moisture vapor penetration and allows the material it protects to be seen, polyethylene film is admirably suited for these applications. The films currently available although termed clear are characterized by a cloudiness, milkiness or haze.
. We have now found that by intimately incorporating and dispersing into a normally solid film-forming ethylene polymer, a minor proportion of polypropylene and there after melt extruding said composition into self-sustaining films, the film obtained is unexpectedly clearer and more transparent than polyethylene film without polypropylene incorporated therein.
In order to effect a uniform improvement in film clarity, it is preferred that a substantially homogeneous mixture of the polypropylene and polyethylene be achieved. Intimate incorporation and dispersioncan be obtained by the use of a differential two-roll mill, a Banbury mixer or similar apparatus. In practice, the polyethylene is introduced into the mill or mixer, the desired amount of polypropylene is added and the two are mechanically worked until a substantially homogeneous mixture is obtained. Best results are obtained by carrying out the incorporation and dispersion of the polypropylene and polyethylene at a temperature equal to or above the melting point of the polyethylene.
Film-forming as used herein denotes a property of polyethylene whereby it can be formed into a self-sustaining film or employed as a surface coating. Any polyethylene which possesses this film-forming property is suitable for use in the composition of our invention. For example, polyethylene with a melt index of 1.9, and a density of 0.918 has given satisfactory results.
Polypropylene, suitable for use in this invention is total polymer made by the process disclosed in Australian patent application No. 6365/55 to Phillips Petroleum Company.
As described therein, the total polymer comprises a tacky portion consisting of low molecular weight polymer, having a weight averaged molecular weight of from 500 to 5000, boiling above 900 F. and soluble at room tem perature in n-pentane and methyl isobutyl ketone; a solid portion consisting of high molecular weight polymer which also boils above 900 F. but which is insoluble in both n-pentane and methyl isobutyl ketone; and 10 to 20% of liquid polymeric material boiling at approximately 400 to 900 F.
The solid portion of the total polymer melts within the range of 240 to 300 F., has a density between about 0.90 and 0.95, and an intrinsic viscosity between about 0.2 and 1.0. The weight averaged molecular weight of the solid polymers ranges from between about 5000 and 20,000. These values were calculated according to the equation wherein M is the weight average molecular weight and N, is the intrinsic viscosity as determined for a solution of 0.2 gram of the polymer in 50 cc. of tetralin at 130 C. This type of molecular weight determination is de-' scribed by Dienis and Klemm, J. Applied Phys, 17, 458 (June 1946).
The proportion of polypropylene in polyethylene is critical. Improved clarity in a film can be obtained without substantially changing other physical characteristics by intimately incorporating and dispersing between 0.1 to 2.0 parts by weight of polypropylene in parts by weight of polyethylene. Amounts of polypropylene added in excess of 2.0 parts, although it improves the clarity of the film has the undesirable effect of imparting to the film a tacky and greasy feel. If an amount of polypropylene less than 0.1 part by weight of polypropylene in 100 parts by weight of polyethylene is used with the method of this invention there is no appreciable improve ment in clarity of the film produced therefrom.
The preferred limits of our invention are 0.5 to 1.5 parts by weight of polypropylene per 100 parts by weight of polyethylene.
Any of the normally employed additives, such as fillers, stabilizers, plasticizers, colorants and the like can be added to the composition of this invention provided they are not present in amounts which will offset the improvement in clarity rendered by the addition of the polypropylene.
The polyethylene-polypropylene mixture after removal from the mill or mixer can be melt extruded by any of the methods known to the art.
This invention is particularly suitable for the production of coatings or non-supported films of polyethylene with a thickness of between less than 0.0005 and about 0.005 in. and is especially useful for production of films for packaging applications where the advantage of transparency is desired in addition to the characteristic properties of polyethylene film such as in food wrapping, sales packages and see-through containers.
In a preferred embodiment of our invention polyethyl ene with a molecular weight above 18,000 is placed on a differential two-roll mill and heated while it is being worked at a temperature equal to or greater than the melting point of the polyethylene i.e., about C.
As soon as the polyethylene begins to soften, the gradual addition of .5 to 1.5 parts by weight of polypropylene per 100 parts by weight of polyethylene is be gun. The operation of the heated mill is not interrupted during the addition and is continued after the addition is completed and a substantially homogeneous mixture is obtained. This mixture is then removed from the mill, cooled and cut into particles of appropriate size for extrusion.
The preferred method of extrusion is the blown tube method disclosed in US. Patent 2,461,975 to Fuller and 2,461,976 to Schenk. This method comprises, in general, dry extruding molten thermoplastic material through an annular die, in the form of a seamless tubing, and as the tubing is being drawn from the die, it is inflated to the desired diameter by means of an air bubble contained therein and a cooling medium applied to the periphery of the tubing. The tubing is drawn continuously from the die and cooled until set whereupon it is flattened and wound on reels. Sheeting can be made from the tubing by cutting one or both of the longitudinal edges.
Film produced from a polyethylene-polypropylene composition prepared without intimate incorporation and dispersion as achieved by heating the polyethylene to at least its melting point, as hereinbefore described does not exhibit the uniformly improved clarity which is characteristic of the composition which has been so processed.
The following examples are illustrative.
EXAMPLE I removed from the mill, cooled and cut intb particles of a size suitable for melt extrusion. The film was formed by the blown tube method of extrusion set forth in US. P. 2,461,976 and the clarity determined by ASTM method D-l003-52. The results of the test are given in terms of total surface haze. The film prepared from the composition containing 0.5 part by weight polypropylene per 100 parts by weight polyethylene had a haze value of 2.1 units.
An additional sample was prepared for control purposes. The above procedure was repeated except that the addition of.polypropylene was omitted. The total surface haze of the film produced in this example was 6.7 units.
EXAMPLE II Example I was repeated except that 1.0 parts by weight of polypropylene added per 100 parts by weight of polyethylene. The total surface haze of the film produced from this composition was found to be 2.6 units. The control sample again had a haze value of 6.7 units.
Tablel Composition. Parts by Weight Haze Value (ASTM D1003-52) Polyethylene Polypropylene Control 100 None 6. 7 Example I.. 100 0. 5 2. 1 Example II... 100 1.0 2. 6
Since it is obvious that various changes and modifications may be made in the above description without departing from the nature or spirit thereof, this invention is not restricted thereto except as set forth in the appended claims.
We claim:
1. A method for the production of polyethylene film which includes the steps of intimately incorporating and dispersing in parts by weight of a normally solid film-forming ethylene polymer 0.1 to 2.0 parts by weight of polypropylene, and thereafter melt extruding the composition.
'2. A method for the production of polyethylene film which includes the steps of intimately incorporating and dispersing in 100 parts by weight of a normally solid film-forming ethylene polymer 0.5 to 1.5 parts by weight of polypropylene, and thereafter melt extruding the composition.
3. The method in claim 1 wherein the polypropylene is intimately incorporated and dispersed in the polyethylene at a temperature at least equal to the melting point of the polyethylene.
- 4. The method in claim 2 wherein the polypropylene is intimately incorporated and dispersed in the po1yethylene at a temperature at least equal to the melting point of the polyethylene.
5. A film-forming composition comprising a homo: geneous mixture of 100 parts by weight of a normally solid film-forming ethylene polymer and 0.1 to 2.0 parts by weight of polypropylene.
6. A film-forming composition comprising a homogeneous mixture of 100 parts by weight of a normally solid ethylene polymer and 05m 1.5 parts by weight of polypropylene.
7. A film-forming composition comprising a homogeneous mixture of 100 parts by weight of a normally solid ethylene polymer having a molecular weight greater than 18,000 and 0.5 to 1.5 parts by weight of polypropylene.
8. A transparent film comprising essentially a homogeneous mixture of 100 parts by weight of a normally solid, film-forming ethylene polymer and 0.1 to 2.0 parts by weight of polypropylene.
9. A transparent film comprising essentially a homogeneous mixture of 100 parts by weight of a normally solid, film-forming ethylene polymer and 0.5 to 1.5 parts by weight of polypropylene.
10. A transparent film comprising essentially a homogeneous mixture of 100 parts by weight of a normally solid, film-forming ethylene polymer having a molecular weight greater than 18,000 and 0.5 to 1.5 parts by weight of polypropylene.
OTHER REFERENCES Raff: Polyethylene, volume XI, (1956), page 71 relied upon.

Claims (1)

  1. 5. A FILM-FORMING COMPOSITION COMPRISING A HOMOGENEOUS MIXTURE OF 100 PARTS BY WEIGHT OF A NORMALLY SOLID FILM-FORMING ETHYLNE POLYMER AND 0.1 TO 2.0 PARTS BYU WEIGHT OF POLYPROPYLENE.
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Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3090770A (en) * 1960-04-26 1963-05-21 Grace W R & Co Blended polyethylene compositions of improved clarity and method of making same
US3137989A (en) * 1959-02-18 1964-06-23 Montedison Spa Dyeable bulky yarns based on polypropylene
US3153681A (en) * 1961-02-13 1964-10-20 Exxon Research Engineering Co Method for blending finely divided polyethylene and polypropylene and extruding the mixture and the product formed thereby
US3192288A (en) * 1961-08-21 1965-06-29 Exxon Research Engineering Co High impact strength blend of isotactic polypropylene, polyethylene and polyisobutylene
US3194850A (en) * 1959-11-13 1965-07-13 Armstrong Cork Co Process of preparing polyethylene resin blends
US3243395A (en) * 1960-12-28 1966-03-29 Eastman Kodak Co Poyethylene modified with polypropylene wax
US3255151A (en) * 1959-09-02 1966-06-07 Argus Chem Stabilization of polypropylene against discoloration
US3256366A (en) * 1959-10-06 1966-06-14 Montedison Spa Process for the preparation and vulcanization of a mixture of an olefin polymer withan olefin copolymer
US3265771A (en) * 1961-02-13 1966-08-09 Exxon Research Engineering Co Polypropylene-polyethylene blends
US3281501A (en) * 1960-03-31 1966-10-25 Exxon Research Engineering Co Low pressure isotactic polypropylene diluted with low pressure linear polyethylene
US3299181A (en) * 1960-05-03 1967-01-17 Eastman Kodak Co Thermally modified polyethylene and other polymers and process for preparing the same
US3355520A (en) * 1964-04-17 1967-11-28 Du Pont Polyolefin blends containing freeradical ethylene polymers and minor amounts of isotactic polypropylene
US3360497A (en) * 1964-10-16 1967-12-26 Hercules Inc Polyolefin pigment dispersion
US3626028A (en) * 1968-05-13 1971-12-07 Elmer J De Witt Thermoplastic, rigid resinous composition and method of making same
US4283459A (en) * 1979-08-09 1981-08-11 E. I. Du Pont De Nemours And Company Insulating composition and articles made therefrom
US5128183A (en) * 1990-08-01 1992-07-07 Borden, Inc. Modified polyolefin film with stable twist retention, dead fold properties and barrier characteristics
US5521251A (en) * 1993-10-20 1996-05-28 Sumitomo Chemical Co., Ltd. Propylene random copolymer composition
US6007666A (en) * 1997-08-20 1999-12-28 General Packaging Products Inc. Process for manufacturing laminated wrapping paper
US6087446A (en) * 1996-03-20 2000-07-11 Hercules Incorporated Masterbatch formulations for polyolefin applications
US6255395B1 (en) 1999-03-22 2001-07-03 Hercules Incorporated Masterbatches having high levels of resin

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2692259A (en) * 1951-04-28 1954-10-19 Standard Oil Co Polymerization of conditioned olefin charging stocks with molybdenum catalysts
US2791576A (en) * 1956-01-12 1957-05-07 Standard Oil Co Process of polymerizing olefins with group 6a oxide

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2692259A (en) * 1951-04-28 1954-10-19 Standard Oil Co Polymerization of conditioned olefin charging stocks with molybdenum catalysts
US2791576A (en) * 1956-01-12 1957-05-07 Standard Oil Co Process of polymerizing olefins with group 6a oxide

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3137989A (en) * 1959-02-18 1964-06-23 Montedison Spa Dyeable bulky yarns based on polypropylene
US3255151A (en) * 1959-09-02 1966-06-07 Argus Chem Stabilization of polypropylene against discoloration
US3256366A (en) * 1959-10-06 1966-06-14 Montedison Spa Process for the preparation and vulcanization of a mixture of an olefin polymer withan olefin copolymer
US3194850A (en) * 1959-11-13 1965-07-13 Armstrong Cork Co Process of preparing polyethylene resin blends
US3281501A (en) * 1960-03-31 1966-10-25 Exxon Research Engineering Co Low pressure isotactic polypropylene diluted with low pressure linear polyethylene
US3090770A (en) * 1960-04-26 1963-05-21 Grace W R & Co Blended polyethylene compositions of improved clarity and method of making same
US3299181A (en) * 1960-05-03 1967-01-17 Eastman Kodak Co Thermally modified polyethylene and other polymers and process for preparing the same
US3243395A (en) * 1960-12-28 1966-03-29 Eastman Kodak Co Poyethylene modified with polypropylene wax
US3265771A (en) * 1961-02-13 1966-08-09 Exxon Research Engineering Co Polypropylene-polyethylene blends
US3153681A (en) * 1961-02-13 1964-10-20 Exxon Research Engineering Co Method for blending finely divided polyethylene and polypropylene and extruding the mixture and the product formed thereby
US3192288A (en) * 1961-08-21 1965-06-29 Exxon Research Engineering Co High impact strength blend of isotactic polypropylene, polyethylene and polyisobutylene
US3355520A (en) * 1964-04-17 1967-11-28 Du Pont Polyolefin blends containing freeradical ethylene polymers and minor amounts of isotactic polypropylene
US3360497A (en) * 1964-10-16 1967-12-26 Hercules Inc Polyolefin pigment dispersion
US3626028A (en) * 1968-05-13 1971-12-07 Elmer J De Witt Thermoplastic, rigid resinous composition and method of making same
US4283459A (en) * 1979-08-09 1981-08-11 E. I. Du Pont De Nemours And Company Insulating composition and articles made therefrom
US5128183A (en) * 1990-08-01 1992-07-07 Borden, Inc. Modified polyolefin film with stable twist retention, dead fold properties and barrier characteristics
US5521251A (en) * 1993-10-20 1996-05-28 Sumitomo Chemical Co., Ltd. Propylene random copolymer composition
US6087446A (en) * 1996-03-20 2000-07-11 Hercules Incorporated Masterbatch formulations for polyolefin applications
US6281290B1 (en) 1996-03-20 2001-08-28 Eastman Chemical Company Compositions, processes for making, and articles of polyolefins, high density polyethylene and hydrocarbon resin
US6007666A (en) * 1997-08-20 1999-12-28 General Packaging Products Inc. Process for manufacturing laminated wrapping paper
US6255395B1 (en) 1999-03-22 2001-07-03 Hercules Incorporated Masterbatches having high levels of resin

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